ASTM D5515-97(2010)e1
(Test Method)Standard Test Method for Determination of the Swelling Properties of Bituminous Coal Using a Dilatometer
Standard Test Method for Determination of the Swelling Properties of Bituminous Coal Using a Dilatometer
SIGNIFICANCE AND USE
Values of the dilatation properties of coals may be used to predict or explain the behavior of a coal or blends during carbonization or in other processes such as gasification, liquefaction, and combustion.
SCOPE
1.1 This test method specifies a procedure for the measurement of the swelling of bituminous coal using a dilatometer.
1.2 The test method is limited in applicability to those coals which have a free swelling index ≥1 as determined in accordance with Test Method D720.
1.3 The values stated in SI units () are to be regarded as standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D5515 − 97 (Reapproved 2010)
Standard Test Method for
Determination of the Swelling Properties of Bituminous Coal
Using a Dilatometer
This standard is issued under the fixed designation D5515; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Added research report information to Section 14 editorially in September 2010.
INTRODUCTION
The principle of this test method is that the final volume of char obtained at the conclusion of a
standard dilatation test is dependent on the mass of coal in the coal pencil and on the radius of the
retort tube.This test method incorporates a procedure which: determines the mass of air-dried coal in
the coal pencil; provides a means to measure the average retort tube radii; and employs a means to
report coal expansion on an air dried coal weight basis.
Other test methods used to determine the swelling properties of bituminous coals include the Ruhr
(ISO 8264) and Audibert-Arnu (ISO 349) International Standard Organization (ISO) test methods.
However these two ISO test methods provide consistently different values for percent dilatation and
percent contraction. Percent contraction and dilatation values obtained using the Audibert-Arnu test
method are higher and lower respectively than those obtained using the Ruhr test method. These
differences have been attributed to trimming the length of the coal pencil from different ends. The
Audibert-Arnu test method specifies that the wider end of the coal pencil be trimmed while the Ruhr
test method specifies that the narrower end of the coal pencil be trimmed.
1. Scope 2. Referenced Documents
1.1 This test method specifies a procedure for the measure- 2.1 ASTM Standards:
ment of the swelling of bituminous coal using a dilatometer. D720Test Method for Free-Swelling Index of Coal
D2013Practice for Preparing Coal Samples for Analysis
1.2 Thetestmethodislimitedinapplicabilitytothosecoals
D2234/D2234MPractice for Collection of a Gross Sample
which have a free swelling index ≥1 as determined in accor-
of Coal
dance with Test Method D720.
IEEE/ASTMSI-10Standard for Use of the International
1.3 The values stated in SI units (IEEE/ASTMSI-10) are to
System of Units (SI): The Modern Metric System
be regarded as standard.
2.2 International Standardization Organization (ISO) Stan-
1.4 This standard does not purport to address all of the dards:
safety concerns, if any, associated with its use. It is the
ISO349 Hard Coal-Audibert-Arnu Dilatometer Test
responsibility of the user of this standard to establish appro-
ISO8264Hard Coal—Determination of the Swelling Prop-
priate safety and health practices and determine the applica-
erties Using a Dilatometer
bility of regulatory limitations prior to use.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method is under the jurisdiction of ASTM Committee D05 on Coal contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
and Coke and is the direct responsibility of Subcommittee D05.15 on Metallurgical Standards volume information, refer to the standard’s Document Summary page on
Properties of Coal and Coke. the ASTM website.
Current edition approved May 1, 2010. Published May 2010. Originally Available from International Organization for Standardization (ISO), 1, ch. de
ε2
approved in 1994. Last previous edition approved in 2004 as D5515–97 (2004) . la Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http://
DOI: 10.1520/D5515-97R10E01. www.iso.ch.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D5515 − 97 (2010)
3. Terminology 3.8 percent dilatation, %D, the maximum recorded height
of char expressed as a percentage, based on an initial coal
3.1 Abbreviations:
pencil height of 60 mm (see Fig. 1).
3.1.1 basement level reference mark height, BLRM , the
ht
char height as measured using the BLRM, after removing the 3.9 softening temperature, T1, the temperature at which the
piston/retort assembly as a unit after completion of the test, height of the coal pencil contracts 1.0% (0.6 mm) from the
expressed in millimetres. highest recorded initial pencil height, expressed in degrees
3.2 coal pencil, a 60-mm-long test specimen formed by Celsius (see Fig. 1).
compressioninamoldfromcoalwhichhasbeenpulverizedto
3.10 wet coal pencil mass, M , the measured mass of a
wet
pass a 250-µm (No. 60) sieve.
trimmed 60-mm-long coal pencil weight, expressed in grams.
3.3 dry coal pencil mass, M , the calculated mass of the
dry
4. Summary of Test Method
trimmed 60-mm-long coal pencil corrected for added water,
expressed in grams. 4.1 The test involves preparing a coal pencil and determin-
ingthechangesofthecoalpencilheightinaretorttubeduring
3.4 equivalentpercentdilatationfor2.50gofairdriedcoal,
a prescribed heating cycle.
%D , the calculated percent expansion for a 2.50-g,
2.50
unmoistened, 60-mm-long, coal pencil corrected for average
5. Significance and Use
tube radii, expressed as a percentage.
5.1 Values of the dilatation properties of coals may be used
3.5 maximum contraction temperature, T2, the temperature
to predict or explain the behavior of a coal or blends during
at which the coal pencil starts swelling, expressed in degrees
carbonization or in other processes such as gasification,
Celsius. For coals which exhibit contraction only, T2 is the
liquefaction, and combustion.
temperature at which the coal pencil reaches its minimum (see
Fig. 1). For coals that exhibit contraction only and are still
6. Apparatus
contracting at 500°C, T2 will be reported as taken at 500°C
6.1 Dilatometer apparatus, a typical arrangement of the
(see Fig. 1d).
dilatometer apparatus is shown in Fig. 2. The apparatus
3.6 maximum dilatation temperature, T3, the temperature at
consists of the following:
which the coal pencil first reaches a maximum height after
6.1.1 Electric Furnace—The dilatometer furnace has a core
swelling, expressed in degrees Celsius (see Fig. 1).
consistingofa65-mm-diametercylindricalblockofaluminum
bronze, resistant to oxidation, and having a sufficiently high
3.7 percent contraction, %C, the minimum recorded height
of char expressed as a percentage, based on an initial coal
pencil height of 60 mm (see Fig. 1).
FIG. 1 Types of Dilatation Curves FIG. 2 Typical Dilatometer Apparatus
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D5515 − 97 (2010)
meltingpoint.Thelengthofthefurnacecorecanvaryfrom400 6.4 Balance—The balance shall have a weighing range of
to 460 mm depending on the length of the retort tubes used. 160.00 g with 0.01-g readability.
The block has three symmetrically placed 15-mm-diameter
bored holes capable of accepting three retort tubes.The core is 7. Preparation of Sample
heated electrically by insulated resistance windings capable of
7.1 Collect a gross sample in accordance with the require-
being controlled at a temperature ramp rate of 3.0 6 0.1°C per
ments of Test Method D2234/D2234M.
minute from within 7 min of the time a test is started to a final
7.2 The analysis sample shall consist of a minimum of 50 g
temperatureof520°C.Thefurnaceshallperforminaccordance
with the specifications outlined in 8.2. The thermocouple used ofcoalpulverizedto250-µm(No.60)sieveinaccordancewith
TestMethodD2013.Performthedilatationanalysisonthecoal
for temperature control is situated in a retort tube placed in the
sample passing 250-µm (No. 60) sieve within five days after
thirdroleofthecore.Thethermocoupletipisplacedincontact
reduction to 250-µm (No. 60) sieve.
with the retort tube wall 60 mm above the bottom of the retort
tube plug.
8. Calibration
6.1.2 System for Measuring Piston Movement and
Temperature—The system shall be capable of measuring the
8.1 For all systems not using a mechanical pen/chart,
linear displacement of the piston to the nearest 1.0 mm and
calibrate the recorder of piston height when there is a differ-
providing a correlation of displacement with temperature.
ence of 3.0 mm or more between the final char heights as
6.1.3 Retort Tube and Pistons—Theretorttubeconsistsofa
calculated from the chart readout and those directly measured
seamlesstubeofsteel,withaninternaldiameterof8.00 60.05
using the BLRM for two consecutive determinations.
mmandanexternaldiameterof14.50 60.05mm.Itshallhave
8.2 The furnace, while being ramped at 3°C per minute,
a support collar at the top and be threaded to accept a gastight,
must meet the following temperature criteria with the empty
threadedplugatitsbase.Theretorttubeshallhaveaminimum
retort tubes placed in Bores 1 and 2 of the furnace and all
length of 345 mm and be supported only by its collar when
temperature measurements made with the thermocouple(s) in
placed in the furnace. The retort tube shall be discarded when
contact with the retort tube wall(s): temperatures measured in
its internal diameter exceeds 8.15 mm.
Bores1and2mustbe 63.0°Cmeasuredatthesameheightfor
6.1.3.1 The piston shall be machined from a steel rod to a
45-mm intervals encompassing the bottom 180 mm; tempera-
finished diameter of 7.80 6 0.05 mm. The piston shall be of
tures between the control thermocouple placed in its usual
sufficient length to permit the mechanical recording or trans-
position and those of Bores 1 and 2 measured at 45-mm
ducer assembly to record a coal pencil height of 30 mm. The
intervalsshallbe 63.0°Cforthebottom135mmand 66°Cfor
piston and mechanical recording or transducer assembly shall
the next 45 mm. The furnace temperature profile shall be
weigh 150 6 10 g. The piston shall be discarded when its
calibrated every twelve months.
diameter is less than 7.65 mm.
8.3 The dilatometer temperature readout of the measuring
6.1.3.2 The piston and retort tube shall be marked and used
thermocouple shall be checked every four months by compari-
as a matched set and require identification imprinted on both
sonwithadigitalthermometerwhichiscalibratedforthesame
the retort tube and its matched piston. A line, called the
type of thermocouple. If the temperature difference is greater
Basement Level Reference Mark (BLRM), shall be imprinted
than 3°C, then the dilatometer furnace temperature readout
on the piston, so when assembled with its matched retort tube,
requires recalibration using a temperature calibrator.
with plug in place, the BLRM is even with the top of the retort
tube.The length from the bottom of the piston to the BLRM is
8.4 Calibrate the retort tubes, as described in Annex A1,
the length of the retort tube bore with plug in place.
every four months.
6.2 Mold and Accessories—The mold and accessories shall
9. Preparation of the Coal Pencil
be capable of producing a 60.0 6 0.5-mm-long coal pencil.
The mold shall have a 70.0 6 0.1-mm inside bore length with
9.1 Allweightsshallberecordedtothenearest0.01g.Care
a taper of 1:50. The narrow end of the bore shall have a
must be taken to avoid sample loss and the following steps
diameterof6.00 60.01mm.Useatrimmingblocktofacilitate
must be performed without a break.
the trimming of the coal pencil to length and the subsequent
9.1.1 Preparation of Homogeneous Coal Sample and Water
weighingofthetrimmedpencil(seeNote1).Theportionofthe
Mix—The amount of water in the mix shall be ≤11 % on a
trimming block holding the pencil shall not weigh more than
weight basis.
155 g.
9.1.1.1 Weigh a mixing vessel. Record the mass as M1.
NOTE 1—The coal pencil may be trimmed to length from either end.
9.1.1.2 Add approximately2gof coal to the pre-weighed
mixingvessel;distributethecoalevenlyoverthebottomofthe
6.3 Cleaning Implements (Recommended)—The cleaning
mixing vessel. Record the mass as M2.
implements for the retort tube consist of an approximately
9.1.1.3 Add approximately 1 mL of distilled water to the
7.95-mm-diameter reamer and a 9-mm bronze wire rifle brush
coal. Record the mass as M3.
with suitable attachments to permit cleaning of the full length
oftheretorttube.Acircularwirebrush,attachedtoabenchtop 9.1.1.4 Mix the coal and water together using a metal
mounted grinder, is recommended for the cleaning of the spatula to form a homogeneous paste. Care must be taken to
pistons. avoid loss of sample.
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D5515 − 97 (2010)
9.1.1.5 Addanotherincrementofapproximately8gofcoal. 12. Calculation
Record the mass as M4. Mix to homogeneity using a metal
12.1 Calculate the percent water added to the coal before
spatula.
pencil making, % , as follows:
H O
9.2 Construction of the Coal Pencil:
% 5 100 3 M3 2M2 / M2 2M1 1 M4 2M3 (1)
@ ~ !# @~ ! ~ !#
H O
9.2.1 Ifamoldreleaseagenthasbeenappliedtotheboreof
thepencilmold,thenexcessreleaseagentmustberemovedby where:
forcing a wad of tissue through the bore of the mold before
% = amount of water added to the coal, %;
H O
adding the moistened coal.
M3 = mass of the mixing vessel plus first coal increment
9.2.2 Addnotlessthantenincrementsofthemoistenedcoal plus water, g;
M2 = mass of the mixing vessel plus first coal increment,
to a mold and compact.
g;
9.2.3 Press the coal pencil out of the mold using equipment
M1 = mass of the mixing vessel, g; and
provided. Gently place the pencil into a trimming block and
M4 = mass of the mixing vessel plus first coal increment
trim the pencil to a 60-mm length. Discard the trimmed off
plus water plus last coal increment, g.
portion of the pencil. Record the mass of the trimmed coal
pencil and trimming block as M5.
12.2 Calculatethemassofthepreparedcoalpencil,M ,as
wet
follows:
9.3 Transfer the trimmed coal pencil into the top of the
horizontally placed retort tube. The coal pencil is gently
M 5 ~M5 2M6! (2)
wet
pushedtothebottomoftheretorttubewiththematchedpiston.
where:
Check that the matched piston slides freely inside the retort
M = mass of the prepared coal pencil, g;
tube.Recordthemassofthetrimmingblockandanyfragments
wet
M5 = mass of the trimmed coal pencil and trimming
ofthetrimmedpencilnottransferredintotheretorttubeasM6.
block, g; and
To determine the accurate mass of coal in the coal pencil, it is
M6 = mass of the trimming block and any untransferred
essentialthatanyuntransferredfragmentsofthecoalpencilare
portion of the coal pencil, g.
weighed along with the trimming block.
12.3 Calculate the mass of air-dried coal in the coal pencil,
10. Procedure
M , as follows:
dry
10.1 Clean the dilatometer retort and piston assembly.
M 5M 2 M 3% 30.01 (3)
~ !
dry wet wet H O
Firmly attach the retort tube plugs to the retort tubes. Check
where:
that the matched piston slides freely in the retort tub
...
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